Sharif Digital Repository

Polyhedral oligomeric silsesquioxanes are 3D nanoscaled materials with large potential in solid phase microextraction (SPME). Here, as a case study, an octaglycidyldimethylsilyl modified polyhedral oligomeric silsesquioxane network is described. It was deposited on a stainless steel wire via a sol–gel method and used as a fiber coating for SPME of aromatic compounds. The uniform pore structure, high surface area, and hydrophobicity of the network make it susceptible toward isolation of non-polar and semi-polar chemical compounds. The performance of the fiber coating was tested with three classes of environmental pollutants, viz. chlorobenzenes (CBs), benzenes (benzene, toluene, ethylbenzene,... 

A polyamidoamine dendrimer was synthesized, placed on magnetite nanoparticles, and the resulting material was then employed as a fiber coating for use in solid phase microextraction of chlorophenols. The polyamidoamine was expected to be an efficient extracting medium due to the presence of multipolar groups and its inner porosity. A thin stainless steel wire was coated with the dendritic polyamidoamine polymer via electrolysis and chemical reactions. The coated fiber was investigated in terms of headspace solid phase microextraction of chlorophenols from aqueous samples followed by GC-MS quantitation. The calibration plots are linear in the 2–1000 ng⋅L−1 chlorophenol concentration ranges.... 

A three–dimensional metal organic framework (3D–MOF) and a two–dimensional polyoxometalate (2D–POM), both incorporating nanostructured molybdenum (VI) oxide, were synthesized and implemented for headspace needle trap extraction of traces of chlorobenzenes (CBs). The 3D–MOF of type {(Mo2O6)(4,4′–bpy)}n and the 2D–POM of type [4,4′–bpy][Mo7O22] were synthesized by a solvothermal process and characterized by FT–IR, powder X–ray diffraction, scanning electron microscopy, transmission electron microscopy, thermogravimetry, energy dispersive X–ray, elemental mapping and Brunner–Emmet–Teller adsorption analyses. The 3D–MOF proved to be superior. Following thermal desorption, the CBs... 

This work introduces a new gradient fiber coating for microextraction of chlorobenzenes. Nanoclusters of organoclay-Cu(II) on a copper wire were fabricated by wireless electrofunctionalization. The resultant gradient coatings are more robust, and thermally and mechanically stable. Wireless electrofunctionalization was carried out in a bipolar cell under a constant deposition potential and using an ethanolic electrolyte solution containing stearic acid and montmorillonite. Stearic acid acts as an inexpensive and green coating while montmorillonite acts as a modifier to impart thermal stability. The gradient morphology of the nanoclusters was investigated by scanning electron microscopy,... 

An attempt was made to combine μ-solid phase extraction and headspace single drop microextraction techniques and use their advantages for trace determination of some volatile organic compounds in aqueous samples. After performing the two-step preconcentration approach, the desired analytes were determined by gas chromatography-mass spectrometry. A resorcinol-formaldehyde-based xerogel was used as the extraction medium in the μ-solid phase extraction (μ-SPE) method. Then, the extracted BTEX was eluted with a rather large amount of methanol. To remove the laborious process including solvent evaporation and further reconstitution, which is usually accompanied by loss of analytes and accuracy,... 

A gradient derived base layer extractive phase was synthesized and applied for the determination of volatile organic compounds (VOCs) in saliva samples using the headspace cooled in–tube microextraction (HS–CITME) method. The base layers from three different sols of phenyltriethoxysilane (PTES), octyltrimethoxysilane (OTMS) and methyltrimethoxysilane (MTMS) as nonpolar precursors were individually dip coated on the stainless steel wires (SSW). Then, the hydrolyzed polar precursor aminopropyltriethoxysilane (APTES) reacted with the silanol groups already formed on the surface of SSWs via controlled rate infusion (CRI) method. The presence of polar and non–polar functional groups on the... 

A headspace adsorptive microextraction technique was developed using a novel polyaniline-nylon-6 (PANI-N6) nanofiber sheet, fabricated by electrospinning. The homogeneity and the porosity of the prepared PANI-N6 sheet were studied using the scanning electron microscopy (SEM) and nanofibers diameters were found to be around 200nm. The novel nanofiber sheet was examined as an extracting medium to isolate some selected chlorobenzenes (CBs), as model compounds, from aquatic media. The extracted analytes were desorbed using μL-amounts of solvent and eventually an aliquot of extractant was injected into gas chromatography-mass spectrometry (GC-MS). Various parameters affecting the extraction and... 

In this paper multivariate response surface methodology (RSM) has been used for the optimization of hydrodistillation-headspace solvent microextraction (HD-HSME) of thymol and carvacrol in Thymus transcaspicus. Quantitative determination of compounds of interest was performed simultaneously using gas chromatography coupled with flame ionization detector (GC-FID). Parameters affecting the extraction efficiency were assessed and the optimized values were 5 min, 2 μL and 3 min for the extraction time, micro-drop volume and cooling time after extraction, respectively. The amounts of analyte extracted increased with plant weight. The calibration curves were linear in the ranges of 6.25-81.25 and... 

A headspace solvent microextraction method was developed for the trace determination of geosmin, an odorant compound, in water samples. After performing the extraction by a microdrop of an organic solvent, the microdrop was introduced directly into a GC-MS injection port. One-at-the-time optimization strategy was applied to investigate and optimize some important extraction parameters such as type of solvent, drop volume, temperature, stirring rate, ionic strength, sample volume, and extraction time. The analytical data exhibited an RSD of less than 5% (n = 5), a linear calibration range of 5-900 ng/L (r2 > 0.998), and a detection limit of 0.8 and 3.3 ng/L using two different sets of... 

Here, a three dimensional nickel–based metal organic framework (MOF) was synthesized via solvothermal and room temperature protocols. In order to study the effects of the synthesis conditions on the physical properties such as pore sizes and shapes of the prepared MOFs, their extraction capabilities were examined. Both MOFs were characterized by Fourier transform infrared spectroscopy, powder X-ray diffraction, scanning electron microscopy, Brunauer–Emmett–Teller and thermogravimetric analyses. Brilliant properties such as porous structure, high surface area and considerable thermal stability make them reasonable candidates to be employed as efficient extractive phases. The efficiency of the... 

A highly efficient polybutylene terephthalate (PBT)-based nanocomposite containing nickel oxide nanoparticles was synthesized by electrospinning technique and used as a fiber coating for solid phase microextraction. The influential morphological parameters and capability of the prepared nanocomposite including the NiO content, the coating time, the PBT concentration and applied voltage were considered for optimization. The applicability of the synthesized fiber coating was examined by headspace solid phase micro extraction and gas chromatography mass spectrometry detection of some volatile organic compounds in aqueous samples. Among the synthesized nanocomposites and pristine PBT nanofibers,... 

A novel method for extraction and analysis of volatile compounds of Artemisia haussknechtii Boiss., using simultaneous hydro-distillation and static headspace liquid microextraction followed by gas chromatography-mass spectrometry (SHD-SHLPME-GCMS) is developed. SHLPME parameters including nature of extracting solvent, headspace volume and design, extraction time, sample weight and microdrop volume were optimized. Comparison of hydro-distillation gas chromatography-mass spectrometry and HD-SHLPME-GCMS showed that the latter method is fast, simple, inexpensive and effective for the analysis of volatile compounds of aromatic plants. By using this method, 56 compounds were extracted and... 

Novel unbreakable solid phase microextraction (SPME) fiber coatings were fabricated by electrospinning method in which the polymeric solution was converted to nanofibers using high voltages. Four different polymers, polyurethane (PU), polycarbonate (PC), polyamide (PA) and polyvinyl chloride (PVC) were prepared as the fiber coatings on thin stainless steel wires. The extraction efficiencies of new coatings were investigated by headspace solid-phase microextraction (HS-SPME) of some environmentally important chlorobenzenes from aqueous samples followed by gas chromatography-mass spectrometry (GC-MS) analysis. Among them, PU showed a prominent efficiency. Effects of coating time and polymer... 

In the present work, the roles of inorganic oxide nanoparticles on the extraction efficiency of polyethylene terephthalate-based nanocomposites were extensively studied. Four fiber coatings based on polyethylene terephthalate nanocomposites containing different types of nanoparticles along with a pristine polyethylene terephthalate polymer were conveniently electrospun on stainless steel wires. The applicability of new fiber coatings were examined by headspace-solid phase microextraction of some environmentally important volatile organic compound such as benzene, toluene, ethylbenzene and xylene (BTEX), as model compounds, from aqueous samples. Subsequently, the extracted analytes were... 

The aim of this study is to introduce an extractive phase based on gradient concept by continuous changing in chemical functional groups for non–targeted analysis. For this purpose, three different two–component coatings containing (3–aminopropyl)trimethoxysilane (APTES) as polar and either phenyltriethoxysilane (PTES), octyl–trimethoxysilane (OTMS) or methyltrimethoxysilane (MTMS) as nonpolar precursors were formed on the modified stainless steel wires using controlled rate infusion (CRI) method. The presence of polar and/or non–polar functional groups on the surface of substrate was evaluated by Fourier–transform infrared spectroscopy (FTIR) together with contact angles determined... 

A new unbreakable solid phase microextraction (SPME) fiber coating based on aniline-silica nanocomposite was electrodeposited on a stainless steel wire. The electropolymerization process was carried out at a constant deposition potential, applied to the corresponding aqueous electrolyte containing aniline and silica nanoparticles. The scanning electron microscopy (SEM) images showed the non-smooth and the porous surface structure of the prepared nanocomposite. The applicability of the new fiber coating was examined by headspace-solid phase microextraction (HS-SPME) of some environmentally important polycyclic aromatic hydrocarbons (PAHs), as model compounds, from aqueous samples.... 

A novel solid phase microextraction (SPME) fiber was fabricated by electrospinning method in which a polymeric solution was converted to nanofibers using high voltages. A thin stainless steel wire was coated by the network of polymeric nanofibers. The polymeric nanofiber coating on the wire was mechanically stable due to the fine and continuous nanofibers formation around the wire with a three dimensional structure. Polyamide (nylon 6), due to its suitable characteristics was used to prepare the unbreakable SPME nanofiber. The scanning electron microscopy (SEM) images of this new coating showed a diameter range of 100-200nm for polyamide nanofibers with a homogeneous and porous surface... 

A headspace solid-phase dynamic extraction (HS-SPDE) technique was developed by the use of polypyrrole (PPy) sorbent, electropolymerized inside the surface of a needle, as a possible alternative to solid-phase microextraction (SPME). Thermal desorption was subsequently, employed to transfer the extracted analytes into the injection port of a gas chromatography-mass spectrometry (GC-MS). The PPy sorbent including polypyrrole-dodecyl sulfate (PPy-DS) was deposited on the interior surface of a stainless steel needle from the corresponding aqueous electrolyte by applying a constant deposition potential. The homogeneity and the porous surface structure of the coating were examined using the...